US6267122B1 - Semiconductor cleaning solution and method - Google Patents
Semiconductor cleaning solution and method Download PDFInfo
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- US6267122B1 US6267122B1 US08/119,785 US11978593A US6267122B1 US 6267122 B1 US6267122 B1 US 6267122B1 US 11978593 A US11978593 A US 11978593A US 6267122 B1 US6267122 B1 US 6267122B1
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- wafer
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- 238000004140 cleaning Methods 0.000 title claims abstract description 14
- 238000000034 method Methods 0.000 title claims description 15
- 239000004065 semiconductor Substances 0.000 title abstract description 5
- 239000004094 surface-active agent Substances 0.000 claims abstract description 5
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 229910052751 metal Inorganic materials 0.000 claims description 13
- 239000002184 metal Substances 0.000 claims description 13
- 239000000908 ammonium hydroxide Substances 0.000 claims description 8
- 229910001868 water Inorganic materials 0.000 claims description 7
- 235000012431 wafers Nutrition 0.000 abstract description 43
- 239000000243 solution Substances 0.000 abstract description 23
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 abstract description 11
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 abstract description 4
- 239000007864 aqueous solution Substances 0.000 abstract description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 abstract 2
- 150000001408 amides Chemical class 0.000 abstract 1
- NRTOMJZYCJJWKI-UHFFFAOYSA-N Titanium nitride Chemical compound [Ti]#N NRTOMJZYCJJWKI-UHFFFAOYSA-N 0.000 description 31
- 239000008367 deionised water Substances 0.000 description 14
- 229910021641 deionized water Inorganic materials 0.000 description 14
- 229920002120 photoresistant polymer Polymers 0.000 description 12
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 9
- 238000005530 etching Methods 0.000 description 9
- 238000000151 deposition Methods 0.000 description 8
- 230000008021 deposition Effects 0.000 description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 description 7
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 7
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 description 7
- 239000010703 silicon Substances 0.000 description 7
- 229910000838 Al alloy Inorganic materials 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 6
- 150000001412 amines Chemical class 0.000 description 6
- 229920005591 polysilicon Polymers 0.000 description 6
- 229910052710 silicon Inorganic materials 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 230000000536 complexating effect Effects 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- 238000011282 treatment Methods 0.000 description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 4
- 238000000206 photolithography Methods 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 239000010936 titanium Substances 0.000 description 4
- 229910052719 titanium Inorganic materials 0.000 description 4
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 description 4
- 238000004506 ultrasonic cleaning Methods 0.000 description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- OEYIOHPDSNJKLS-UHFFFAOYSA-N choline Chemical compound C[N+](C)(C)CCO OEYIOHPDSNJKLS-UHFFFAOYSA-N 0.000 description 3
- 229960001231 choline Drugs 0.000 description 3
- 239000004020 conductor Substances 0.000 description 3
- 239000000356 contaminant Substances 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 229910021332 silicide Inorganic materials 0.000 description 3
- 229910021341 titanium silicide Inorganic materials 0.000 description 3
- AVFZOVWCLRSYKC-UHFFFAOYSA-N 1-methylpyrrolidine Chemical compound CN1CCCC1 AVFZOVWCLRSYKC-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- 241000252506 Characiformes Species 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 2
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 2
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 description 2
- AHVYPIQETPWLSZ-UHFFFAOYSA-N N-methyl-pyrrolidine Natural products CN1CC=CC1 AHVYPIQETPWLSZ-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000003929 acidic solution Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000003637 basic solution Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 239000000460 chlorine Substances 0.000 description 2
- 229910052801 chlorine Inorganic materials 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 238000011065 in-situ storage Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000004544 sputter deposition Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- 229910015844 BCl3 Inorganic materials 0.000 description 1
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- CYTYCFOTNPOANT-UHFFFAOYSA-N Perchloroethylene Chemical group ClC(Cl)=C(Cl)Cl CYTYCFOTNPOANT-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- -1 aluminum hydrocarbon silicates Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000006117 anti-reflective coating Substances 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 238000004380 ashing Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- WCCJDBZJUYKDBF-UHFFFAOYSA-N copper silicon Chemical compound [Si].[Cu] WCCJDBZJUYKDBF-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 238000005441 electronic device fabrication Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 238000005755 formation reaction Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 238000005468 ion implantation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 150000003141 primary amines Chemical class 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 125000001453 quaternary ammonium group Chemical group 0.000 description 1
- 230000003134 recirculating effect Effects 0.000 description 1
- 238000005201 scrubbing Methods 0.000 description 1
- 150000003335 secondary amines Chemical class 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 125000006850 spacer group Chemical group 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- FAQYAMRNWDIXMY-UHFFFAOYSA-N trichloroborane Chemical compound ClB(Cl)Cl FAQYAMRNWDIXMY-UHFFFAOYSA-N 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Images
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
- H01L21/3205—Deposition of non-insulating-, e.g. conductive- or resistive-, layers on insulating layers; After-treatment of these layers
- H01L21/321—After treatment
- H01L21/3213—Physical or chemical etching of the layers, e.g. to produce a patterned layer from a pre-deposited extensive layer
- H01L21/32133—Physical or chemical etching of the layers, e.g. to produce a patterned layer from a pre-deposited extensive layer by chemical means only
- H01L21/32135—Physical or chemical etching of the layers, e.g. to produce a patterned layer from a pre-deposited extensive layer by chemical means only by vapour etching only
- H01L21/32138—Physical or chemical etching of the layers, e.g. to produce a patterned layer from a pre-deposited extensive layer by chemical means only by vapour etching only pre- or post-treatments, e.g. anti-corrosion processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
- B08B3/04—Cleaning involving contact with liquid
- B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
- B08B3/12—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration by sonic or ultrasonic vibrations
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
- C11D7/02—Inorganic compounds
- C11D7/04—Water-soluble compounds
- C11D7/06—Hydroxides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02041—Cleaning
- H01L21/02057—Cleaning during device manufacture
- H01L21/0206—Cleaning during device manufacture during, before or after processing of insulating layers
- H01L21/02063—Cleaning during device manufacture during, before or after processing of insulating layers the processing being the formation of vias or contact holes
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
- H01L21/3205—Deposition of non-insulating-, e.g. conductive- or resistive-, layers on insulating layers; After-treatment of these layers
- H01L21/321—After treatment
- H01L21/3213—Physical or chemical etching of the layers, e.g. to produce a patterned layer from a pre-deposited extensive layer
- H01L21/32133—Physical or chemical etching of the layers, e.g. to produce a patterned layer from a pre-deposited extensive layer by chemical means only
- H01L21/32134—Physical or chemical etching of the layers, e.g. to produce a patterned layer from a pre-deposited extensive layer by chemical means only by liquid etching only
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D2111/00—Cleaning compositions characterised by the objects to be cleaned; Cleaning compositions characterised by non-standard cleaning or washing processes
- C11D2111/10—Objects to be cleaned
- C11D2111/14—Hard surfaces
- C11D2111/22—Electronic devices, e.g. PCBs or semiconductors
Definitions
- the invention relates to electronic device fabrication, and, more particularly, to semiconductor cleaning.
- Fabrication of integrated circuits on a wafer of semiconductor material such as silicon typically involves sequences of processing steps such as masked introduction of dopants (impurities effecting electrical characteristics) by ion implantation or diffusion, formation of insulating layers by oxidation or deposition followed by masked etching to make patterns, and formation of conductors by deposition of polycrystalline silicon (polysilicon) or metals also followed by masked etching to make patterns. And prior to each of these steps affecting the wafer surface, the surface must be cleaned to get rid of process chemicals from the prior steps in order to insure that the prescribed reaction occurs or the prescribed material interface arises. Contaminants and irregularities can affect electrical behavior, and cleanups may themselves introduce contaminants including heavy metals, alkali metals and light elements. Cleanups may also be the source of submicron sized particulates that are difficult to detect.
- Wafer cleanups should remove gross organics and particulates, remove organic films, remove surface-adsorbed ions and plated metal contaminants, and sometimes remove surface oxide.
- Standard wafer cleanups include mechanical scrubbing in a liquid and ultrasonic agitation in deionized water (particulate removal), chemical cleaners such as solutions of “piranha” and “RCA cleanup” and choline cleanup, and dry cleaners such as ozone with ultraviolet light.
- Piranha is a solution of hydrogen peroxide (H 2 O 2 ) and sulffric acid (H 2 SO 4 )
- choline cleanup uses a solution of H 2 O 2 with choline ((CH 3 ) 3 N(CH 2 CH 2 OH)OH) at 50° C.
- RCA cleanup has up to three steps: first a removal of gross organics with perchloroethylene, next a removal of residual organic films with a basic solution of H 2 O 2 and NH 4 OH followed by deionized water rinse and spin dry, and lastly a removal of metallics with an acidic solution of H 2 O 2 and HCl again followed a deionized water rinse and spin dry.
- the solutions are used at 75-80° C. and essentially provide an oxidizing and complexing treatment which does not attack silicon or silicon dioxide (oxide).
- the basic solution cleanup alone is frequently called SC-1 and the acidic solution cleanup alone is called SC-2.
- the present invention provides ammonia and other amine solutions as a metallized wafer cleaner. These solutions may be used with ultrasonic cleaning, or alone and heated, or with both heated, ultrasonic cleaning.
- FIGS. 1-8 illustrate in cross sectional elevation view process steps including a first preferred embodiment method of cleaning.
- FIG. 9 shows an ultrasonic bath.
- FIGS. 1-4 illustrate in cross sectional elevation views steps in silicon semiconductor wafer processing which include a first preferred embodiment method of wafer cleaning for wafers with exposed patterned metal.
- FIG. 1 shows the wafer after deposition of aluminum alloy layer 106 with cladding TiN layers 102 - 103 on either side
- Aluminum alloy 106 may be an alloy such as 1 ⁇ 2% silicon-copper (Al:Si:Cu) or 1 ⁇ 2% copper (Al:Cu); the bottom TiN layer 102 acts as a diffusion barrier to prevent aluminum 106 reaction with underlying items such as the tungsten plug 108 , and the top TiN layer 103 acts as an antireflective coating to aid in the photolithography of the following steps.
- Tungsten plug 108 extends through an underlying oxide insulation layer 107 and provides vertical conductor connection.
- the TiN layers 102 - 103 typically will be on the order of 0.05 ⁇ m thick and deposited by chemical vapor deposition (CVD) or by reactive ion sputtering.
- the aluminum alloy layer typically will be on the order of 0.5 to 1 ⁇ m thick and deposited by sputtering.
- Particulate sources include the deposition chamber walls, the vacuum pumping system, and other sources such as the wafer handling and inspection.
- the first preferred embodiment method dips the metallized wafer in a bath of aqueous NH 4 OH at a temperature in the range of about 25-90° C. for from about five to twenty-five minutes. This solution does not attack TiN and provides particulate removal superior to a deionized water rinse. After the dip in NH 4 OH, rinse the wafer with deionized water in a batch mode rinse tank or in a single wafer rinser to remove any traces of the NH 4 OH before drying.
- the next processing steps pattern the TiN clad aluminum alloy into conducting lines (interconnects) and include photolithography.
- photolithography by spinning photoresist onto the cleaned wafer.
- reactive ion etch RIE
- Chlorine-based etches such as BCl 3 plus Cl 2 may be used. This etching creates a multitude of residues and particulates as illustrated heuristically in FIG. 2 . in particular, the RIE creates residue 112 on the sidewalls of patterned photoresist 110 and etched aluminum alloy 106 .
- Sidewall residue 112 typically includes inorganics such as aluminum hydrocarbon silicates and aluminum or titanium containing organic polymer chains depending upon the type of photoresist and etch chemistry used. Particulates such as 114 on the horizontal surfaces also arise and may have their sources in sidewall residue 112 or from etch by-products which accumulate in the etch equipment and get transferred to the wafer.
- the RIE creates numerous particulates of sizes in the range of 0.1-1.0 ⁇ m which are large enough to be fatal defects for processes with linewidths below 1 ⁇ m if located in critical areas but are small enough to be difficult to remove.
- the photoresist 110 is removed by an in-situ oxygen plasma (ash), by a dedicated oxygen asher, by solvent immersion, or by a combination of these. In-situ ashing is preferred because the wafer need not be removed from the etching chamber after the metal etch. Photoresist removal leaves the sidewall residue in tact, although oxidized and perhaps with more particulates dispersed on the patterned metal and the underlying exposed oxide as illustrated in FIG. 3 .
- ash in-situ oxygen plasma
- the preferred embodiment method cleans the etched and ashed wafer by first immersing in a solvent or by applying an RF vapor treatment. This removes the bulk of the etching residue. Next, again dip the metallized wafer in a bath of aqueous NH 4 OH at a temperature in the range of about 25-90° C. for from about five to twenty-five minutes. After the dip in NH 4 OH, rinse the wafer with deionized water in a batch mode rinse tank or in a single wafer rinser to remove any traces of the NH 4 OH before drying.
- FIG. 4 illustrates the cleaned wafer.
- the thus cleaned wafer is ready for deposition of the next insulation layer and, perhaps further metal layers.
- the cleanings with NH 4 OH provide better particulate removal than ultrasonic deionized water, and this may be due to the complexing power of the ammonium ion with metals and to improved wetability.
- the volume ratio of NH 4 OH to H 2 O in the solution could be from 0.0001 to 0.2 and still provide good results, although a ratio of 0.1 may be most convenient.
- FIGS. 5-8 illustrate the use of the first preferred embodiment cleaning method for local interconnects in silicided silicon integrated circuits.
- FIG. 5 shows in cross sectional elevation view part of a CMOS integrated circuit during processing with polysilicon insulated gate 502 having sidewall spacer 504 and located on silicon substrate 510 between doped source 512 and drain 514 and with polysilicon first level interconnect 522 located on field oxide 520 .
- the next processing step deposits a conformal layer of titanium metal (4-90 nm thick) and reacts the titanium with abutting silicon to form titanium silicide (TiSi 2 ) in furnace or rapid thermal annealer at 400-1000° C. for 1-60 minutes.
- FIG. 6 shows silicide 622 formed on polysilicon interconnect 522 , silicide 602 on polysilicon gate 502 , silicide 612 and 614 on source 512 and drain 514 , and TiN 620 elsewhere.
- FIG. 6 also illustrates particulates 609 generated during the titanium deposition and the subsequent silicidation-nitridation reaction.
- the first preferred method of cleaning with an aqueous solution of NH 4 OH and deionized water rinse again removes particulates 609 . That is, dip the wafer in a bath of aqueous NH 4 OH at a temperature in the range of about 25-90° C. for from about five to twenty-five minutes. After the dip in NH 4 OH, rinse the wafer with deionized water in a batch mode rinse tank or in a single wafer rinser to remove any traces of the NH 4 OH before drying.
- FIG. 7 illustrates etched TiN 620 as forming a local interconnect from silicided polysilicon interconnection 522 - 622 to silicided drain 514 - 614 plus the residue 712 and particulates 714 .
- strip or ash photoresist 710 which will generate more particulates and leave the residues although perhaps in a oxidized form, and then remove the residues with a solvent rinse or a vapor HF treatment, generating more particulates.
- strip or ash photoresist 710 again dip the metallized wafer in a bath of aqueous NH 4 OH at a temperature in the range of about 25-90° C. for from about five to twenty-five minutes.
- FIG. 8 shows the cleaned wafer with local interconnections ready for a deposition of a layer of insulation.
- FIG. 9 heuristically shows in cross sectional elevation view an ultrasonic bath with a transducer, a recirculating pump plus filter and heater, and a wafer holder full of wafers to be cleaned.
- a power oscillator drives the transducer at 500-1500 KHz which couples this energy into the bath NH 4 OH solution.
- the ultrasonic energy helps the bath solution dislodge particulates.
- the bath solution again is aqueous NH 4 OH at a temperature in the range of about 25-90° C. and again wafers are kept from about five to twenty-five minutes in the bath with application of ultrasonic energy.
- This ultrasonic cleaning step may be substituted for the hot NH 4 OH dip of the first preferred embodiment and may use the same concentrations of NH 4 OH.
- the third preferred embodiment also cleans metallized wafers, but with a quarternary ammonium ion in place of the NH 4 + of the fist two preferred embodiments.
- a solution of N(CH 3 ) 4 OH tetramethylammonium hydroxide
- NR 1 R 2 R 3 R 4 OH tetramethylammonium hydroxide
- each R j is an alkyl or aryl group.
- the larger substitutions have the advantage of adjusting either solution wettability or complexing power.
- the larger substituted groups also imply flammability and limit the use of the solution in an ultrasonic bath.
- a broad concentration range such as a volume ratio of substituted quarternary ammnomium hydroxide to water of 0.0001 to 0.2, should provide good results.
- mixtures of ammonium hydroxide and various quaternary ammonium hydroxides could be used.
- the fourth preferred embodiment also cleans metallized wafers with a more generic compound replacing the ammonium hydroxide of the first two preferred embodiments.
- the complexing power of the nitrogen in ammonium hydroxide also appears in amines (compounds with an NH 2 functional group) such as ethylenediamine (NH 2 CH 2 CH 2 NH 2 ) and these amines also do not attack TiN or TiSi 2 .
- ethylenediamine chelates various metal ions to aid cleaning.
- the fifth preferred embodiment uses any of the solutions of the first four preferred embodiment in conjuction with a surfactant to enhance particulate removal.
- Surfactant such as NCW- 601 typically include hydrophilic functional groups and have limited use in ultrasonic treatments.
- the preferred embodiments may be used over a large range of concentrations, treatment times, and bath temperatures depending upon the particular demands, including solution lifetime, throughput, and cost. For example, treatment times from 15 seconds to several hours may be used; higher temperatures may be used in pressurized systems; and solutions of mixtures of various amines and ammonium hydroxide plus surfactants could be used.
- ammonium or amine solutions for cleaning wafers with exposed TiN include the wetting and complexing in hot solutions with possible ultrasonic power to remove particulates without the TiN attack of peroxide solutions.
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Abstract
An ammonium or amide aqueous solution without oxidzers for cleaning semiconductor wafers with exposed TiN (103). Effective particulate (109) removal occurs without the standard use of hydrogen peroxide which would attack the TiN (103). Solution temperatures up to 90° C. plus applied ultrasonic energy enhance the cleaning efficiency. Surfactants may be included.
Description
The invention relates to electronic device fabrication, and, more particularly, to semiconductor cleaning.
Fabrication of integrated circuits on a wafer of semiconductor material such as silicon typically involves sequences of processing steps such as masked introduction of dopants (impurities effecting electrical characteristics) by ion implantation or diffusion, formation of insulating layers by oxidation or deposition followed by masked etching to make patterns, and formation of conductors by deposition of polycrystalline silicon (polysilicon) or metals also followed by masked etching to make patterns. And prior to each of these steps affecting the wafer surface, the surface must be cleaned to get rid of process chemicals from the prior steps in order to insure that the prescribed reaction occurs or the prescribed material interface arises. Contaminants and irregularities can affect electrical behavior, and cleanups may themselves introduce contaminants including heavy metals, alkali metals and light elements. Cleanups may also be the source of submicron sized particulates that are difficult to detect.
Wafer cleanups should remove gross organics and particulates, remove organic films, remove surface-adsorbed ions and plated metal contaminants, and sometimes remove surface oxide. Standard wafer cleanups include mechanical scrubbing in a liquid and ultrasonic agitation in deionized water (particulate removal), chemical cleaners such as solutions of “piranha” and “RCA cleanup” and choline cleanup, and dry cleaners such as ozone with ultraviolet light. Piranha is a solution of hydrogen peroxide (H2O2) and sulffric acid (H2SO4), and choline cleanup uses a solution of H2O2 with choline ((CH3)3N(CH2CH2OH)OH) at 50° C. followed by an ultrasonic clean in deionized water and a deionized water rinse plus spin dry. RCA cleanup has up to three steps: first a removal of gross organics with perchloroethylene, next a removal of residual organic films with a basic solution of H2O2 and NH4OH followed by deionized water rinse and spin dry, and lastly a removal of metallics with an acidic solution of H2O2 and HCl again followed a deionized water rinse and spin dry. The solutions are used at 75-80° C. and essentially provide an oxidizing and complexing treatment which does not attack silicon or silicon dioxide (oxide). The basic solution cleanup alone is frequently called SC-1 and the acidic solution cleanup alone is called SC-2.
Current cleanup systems typically rely on the RCA cleanup as a pre-furnace cleanup. However, once a wafer has been metallized, then both the SC-1 and SC-2 cleanups must be abandoned in favor of other cleaners in order to avoid etching desired metal. The recent use of titanium nitride (TiN) cladding for aluminum or for coated contacts, gates, and emitters or as a standalone “local interconnect” conductor has created a problem in that both the SC-1 basic cleanup and the SC-2 acidic cleanup attack TiN. Thus cleanup for metallized wafers relies on solvents, such as N-methylpyrrolidine (NMP), or ultrasonic or spin rinse cleaning with deionized water. (Note that many organic solvents are flammable and thus cannot be used in ultrasonic cleaning baths due to the potential for explosion). But these cleanups have limited efficacy, and there is a need for better cleanups for metallized wafers, especially with exposed TiN.
The present invention provides ammonia and other amine solutions as a metallized wafer cleaner. These solutions may be used with ultrasonic cleaning, or alone and heated, or with both heated, ultrasonic cleaning.
The drawings are schematic for clarity.
FIGS. 1-8 illustrate in cross sectional elevation view process steps including a first preferred embodiment method of cleaning.
FIG. 9 shows an ultrasonic bath.
First Preferred Embodiment
FIGS. 1-4 illustrate in cross sectional elevation views steps in silicon semiconductor wafer processing which include a first preferred embodiment method of wafer cleaning for wafers with exposed patterned metal. In particular, FIG. 1 shows the wafer after deposition of aluminum alloy layer 106 with cladding TiN layers 102-103 on either side Aluminum alloy 106 may be an alloy such as ½% silicon-copper (Al:Si:Cu) or ½% copper (Al:Cu); the bottom TiN layer 102 acts as a diffusion barrier to prevent aluminum 106 reaction with underlying items such as the tungsten plug 108, and the top TiN layer 103 acts as an antireflective coating to aid in the photolithography of the following steps. Tungsten plug 108 extends through an underlying oxide insulation layer 107 and provides vertical conductor connection. The TiN layers 102-103 typically will be on the order of 0.05 μm thick and deposited by chemical vapor deposition (CVD) or by reactive ion sputtering. The aluminum alloy layer typically will be on the order of 0.5 to 1 μm thick and deposited by sputtering.
The surface of the top TiN 103 attracts particulates, heuristically illustrated by particulates 109 in FIG. 1, at the final stages of the TiN deposition and characterizations, during transfer of the wafer for the following photolithography steps, and also during the etching of the TiN clad aluminum alloy. Particulate sources include the deposition chamber walls, the vacuum pumping system, and other sources such as the wafer handling and inspection.
To clean the top TiN surface of particulates, the first preferred embodiment method dips the metallized wafer in a bath of aqueous NH4OH at a temperature in the range of about 25-90° C. for from about five to twenty-five minutes. This solution does not attack TiN and provides particulate removal superior to a deionized water rinse. After the dip in NH4OH, rinse the wafer with deionized water in a batch mode rinse tank or in a single wafer rinser to remove any traces of the NH4OH before drying.
Typically, the next processing steps pattern the TiN clad aluminum alloy into conducting lines (interconnects) and include photolithography. Thus begin the photolithography by spinning photoresist onto the cleaned wafer. Next, expose and develop a pattern in the photoresist to define the desired interconnects to be made from the deposited metal. Then reactive ion etch (RIE) the deposited metal using the patterned photoresist as the etch mask. Chlorine-based etches such as BCl3 plus Cl2 may be used. This etching creates a multitude of residues and particulates as illustrated heuristically in FIG. 2. in particular, the RIE creates residue 112 on the sidewalls of patterned photoresist 110 and etched aluminum alloy 106. Sidewall residue 112 typically includes inorganics such as aluminum hydrocarbon silicates and aluminum or titanium containing organic polymer chains depending upon the type of photoresist and etch chemistry used. Particulates such as 114 on the horizontal surfaces also arise and may have their sources in sidewall residue 112 or from etch by-products which accumulate in the etch equipment and get transferred to the wafer. The RIE creates numerous particulates of sizes in the range of 0.1-1.0 μm which are large enough to be fatal defects for processes with linewidths below 1 μm if located in critical areas but are small enough to be difficult to remove.
Next, the photoresist 110 is removed by an in-situ oxygen plasma (ash), by a dedicated oxygen asher, by solvent immersion, or by a combination of these. In-situ ashing is preferred because the wafer need not be removed from the etching chamber after the metal etch. Photoresist removal leaves the sidewall residue in tact, although oxidized and perhaps with more particulates dispersed on the patterned metal and the underlying exposed oxide as illustrated in FIG. 3.
The preferred embodiment method cleans the etched and ashed wafer by first immersing in a solvent or by applying an RF vapor treatment. This removes the bulk of the etching residue. Next, again dip the metallized wafer in a bath of aqueous NH4OH at a temperature in the range of about 25-90° C. for from about five to twenty-five minutes. After the dip in NH4OH, rinse the wafer with deionized water in a batch mode rinse tank or in a single wafer rinser to remove any traces of the NH4OH before drying. FIG. 4 illustrates the cleaned wafer.
The thus cleaned wafer is ready for deposition of the next insulation layer and, perhaps further metal layers. The cleanings with NH4OH provide better particulate removal than ultrasonic deionized water, and this may be due to the complexing power of the ammonium ion with metals and to improved wetability. The volume ratio of NH4OH to H2O in the solution could be from 0.0001 to 0.2 and still provide good results, although a ratio of 0.1 may be most convenient.
FIGS. 5-8 illustrate the use of the first preferred embodiment cleaning method for local interconnects in silicided silicon integrated circuits. In particular, FIG. 5 shows in cross sectional elevation view part of a CMOS integrated circuit during processing with polysilicon insulated gate 502 having sidewall spacer 504 and located on silicon substrate 510 between doped source 512 and drain 514 and with polysilicon first level interconnect 522 located on field oxide 520. The next processing step deposits a conformal layer of titanium metal (4-90 nm thick) and reacts the titanium with abutting silicon to form titanium silicide (TiSi2) in furnace or rapid thermal annealer at 400-1000° C. for 1-60 minutes. A nitrogen atmosphere during the reaction prevents silicon migration through the metal by forming TiN in a competing reaction. FIG. 6 shows silicide 622 formed on polysilicon interconnect 522, silicide 602 on polysilicon gate 502, silicide 612 and 614 on source 512 and drain 514, and TiN 620 elsewhere. FIG. 6 also illustrates particulates 609 generated during the titanium deposition and the subsequent silicidation-nitridation reaction.
The first preferred method of cleaning with an aqueous solution of NH4OH and deionized water rinse again removes particulates 609. That is, dip the wafer in a bath of aqueous NH4OH at a temperature in the range of about 25-90° C. for from about five to twenty-five minutes. After the dip in NH4OH, rinse the wafer with deionized water in a batch mode rinse tank or in a single wafer rinser to remove any traces of the NH4OH before drying.
After cleaning, spin on and pattern photoresist to define local interconnections to be made from the TiN layer 620. Then use the patterned photoresist as an etch mask to etch the TiN, either with a chlorine plasma etch or a wet etch with NH4OH+H2O2+H2O (which are the same ingredients as SC-1). As with the previously described etching of TiN-clad aluminum, the etching will leave residues 712 on the sidewalls of photoresist 710 and TiN 620 and particulates 714 elsewhere. The residues and particulates may derive from the photoresist plus TiN being etched plus the etchant. FIG. 7 illustrates etched TiN 620 as forming a local interconnect from silicided polysilicon interconnection 522-622 to silicided drain 514-614 plus the residue 712 and particulates 714.
Again as with the TiN-clad aluminum etch, strip or ash photoresist 710, which will generate more particulates and leave the residues although perhaps in a oxidized form, and then remove the residues with a solvent rinse or a vapor HF treatment, generating more particulates. Lastly, again dip the metallized wafer in a bath of aqueous NH4OH at a temperature in the range of about 25-90° C. for from about five to twenty-five minutes. After the dip in NH4OH, rinse the wafer with deionized water in a batch mode rinse tank or in a single wafer rinser to remove any traces of the NH4OH before drying. FIG. 8 shows the cleaned wafer with local interconnections ready for a deposition of a layer of insulation.
Second Preferred Embodiment
The second preferred embodiment also cleans metallized wafers with an NH4OH solution, but with the use of ultrasonic energy. In particular, FIG. 9 heuristically shows in cross sectional elevation view an ultrasonic bath with a transducer, a recirculating pump plus filter and heater, and a wafer holder full of wafers to be cleaned. A power oscillator drives the transducer at 500-1500 KHz which couples this energy into the bath NH4OH solution. The ultrasonic energy helps the bath solution dislodge particulates. The bath solution again is aqueous NH4OH at a temperature in the range of about 25-90° C. and again wafers are kept from about five to twenty-five minutes in the bath with application of ultrasonic energy. After the ultrasonic-assisted dip in NH4OH, rinse the wafer with deionized water in a batch mode rinse tank or in a single wafer rinser to remove any traces of the NH4OH before drying. This ultrasonic cleaning step may be substituted for the hot NH4OH dip of the first preferred embodiment and may use the same concentrations of NH4OH.
Third Preferred Embodiment
The third preferred embodiment also cleans metallized wafers, but with a quarternary ammonium ion in place of the NH4 + of the fist two preferred embodiments. In particular, a solution of N(CH3)4OH (tetramethylammonium hydroxide) could be used at 25-90° C. in place of the NH4OH of the first and second preferred embodiments. More generally, a generic quarternary ammonium hydroxide, NR1R2R3R4OH, could be used where each Rj is an alkyl or aryl group. The larger substitutions have the advantage of adjusting either solution wettability or complexing power. However, the larger substituted groups also imply flammability and limit the use of the solution in an ultrasonic bath. Again, a broad concentration range, such as a volume ratio of substituted quarternary ammnomium hydroxide to water of 0.0001 to 0.2, should provide good results. Also, mixtures of ammonium hydroxide and various quaternary ammonium hydroxides could be used.
Fourth Preferred Embodiment
The fourth preferred embodiment also cleans metallized wafers with a more generic compound replacing the ammonium hydroxide of the first two preferred embodiments. In particular, the complexing power of the nitrogen in ammonium hydroxide also appears in amines (compounds with an NH2 functional group) such as ethylenediamine (NH2CH2CH2NH2) and these amines also do not attack TiN or TiSi2. Indeed, ethylenediamine chelates various metal ions to aid cleaning. Thus primary, secondary, and tertiary amines (and hydrazes which resemble amines) such as methylamine (N(CH3)H2), dimethylamine (N(CH3)2H), and trimethylamine (N(CH3)3), respectively, with low molecular weight are water soluble and could be used in place of or in conjunction with the (quaternary) ammonium hydroxide(s) of the foregoing embodiments. Again, with increasing hydrocarbon character, the solutions have limited ultrasonic bath use.
Fifth Preferred Embodiment
The fifth preferred embodiment uses any of the solutions of the first four preferred embodiment in conjuction with a surfactant to enhance particulate removal. Surfactant such as NCW-601 typically include hydrophilic functional groups and have limited use in ultrasonic treatments.
Modifications and Advantages
The preferred embodiments may be used over a large range of concentrations, treatment times, and bath temperatures depending upon the particular demands, including solution lifetime, throughput, and cost. For example, treatment times from 15 seconds to several hours may be used; higher temperatures may be used in pressurized systems; and solutions of mixtures of various amines and ammonium hydroxide plus surfactants could be used.
The advantages of the ammonium or amine solutions for cleaning wafers with exposed TiN include the wetting and complexing in hot solutions with possible ultrasonic power to remove particulates without the TiN attack of peroxide solutions.
Claims (5)
1. A method of wafer cleaning, comprising the steps of:
(a) providing a wafer to be cleaned, said wafer with exposed metal regions; and
(b) applying a solution consisting essentially of water plus ammonium hydroxide to said wafer while simultaneously applying an ultrasonic energy to said solution.
2. The method of claim 1, further comprising the step of:
(a) after step (b) of claim 1, rinsing said wafer with water.
3. The method of claim 1, wherein:
(a) said step of applying includes the step of adding a surfactant to the solution.
4. The method of claim 1, wherein:
(a) said solution has a temperature in the range of 25-90° C.
5. The method of claim 1, wherein:
(a) the ratio of ammonium hydroxide to water is in the range of 0.001 to 0.2.
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